Stabilized iron carbonyl



Patented July 4, 1950 UNITED" STATES PATENT OFFICE STABILIZED IRON CARBONYL Robert E. Christ, Elizabeth, N. J assignor to General Aniline & Film Corporation, New York, N. Y., a corporation of Delaware No Drawing. Application December 30, 1947, Serial No. 794,785

. nous black precipitate of ferrous oxide and other iron compounds.

I have found that the stability of iron carbonyl I to light can be materially improved by the admixture therewith of a talloil soap composition containing an aliphatic alcohol of at least 3 carbon atoms.

The talloil soap compositions useful in accordance with the invention for improving the stability of iron carbonyl are such as are obtainable by saponifying talloil in successive partial saponiflcations in the presence of an aliphatic alcohol of at least 3 carbon atoms as diluent for the reaction, with, on the one hand, polyalkylen polyamines, such as diethylene triamine, triethylene tetramine, tetraethylene pentamine, or hydroxyalkyl alkylene polyamines, such as hydroxyethyl ethylenediamine, N,N di(2 hydroxyethyl) trimethylene diamine, and the like, and with potassium hydroxide, on the other, partial saponification with the amine occurring first followed by completion of the saponification with the potassium hydroxide.

The mixed talloil soap products are neutral to alkaline soaps with which is mixed the aliphatic alcohol employed as diluent in the saponification reaction. In consistency they may Vary from easily pounable liquids to soft pastes in which the proportions of the potassium soap and of the polyalkylene polyamine or hydroxyalkyl alkylene polyamine soap can be varied within a wide range, for example, from 1 part potassium soap to 99 parts of the amine soap and in the opposite relationship.

For effecting stabilization of the iron carbonyl to the action of light, the potassium-amine talloil soap compositions can beemployed in widely varying amounts, the particular quantit used depending on the efficacy, of the individual soap compositions and on the degree of stability desired in the iron carbonyl. Generally, proportions of the soap compositions equal to form 5% to 50% by volume on the iron carbonyl will sufllce 2 to effect a marked improvement in the stabili y of the iron carbonyl to light.

The mixed talloil soap compositions are added to the iron carbonyl, which he liquid, by a'simple but efllcient stirring operation, an organic solvent for the iron carbonyl which is also a solvent for the soap composition being employed for blending of the ingredients. The iron' carbonyl may be dissolved in the organic solvent and the soap composition added thereto or the order may be reversed with addition of the solvent solu:

tion of the soap composition to the iron carbonyl. Blending agents may be selected from among such common organic solvents as gasoline, kerosene, benzene, isopropanol, butanol and acetone. Gasoline, kerosene or benzene can be used for blending of the talloil soap compositions having a potassium soap content in the higher ranges.

Talloil is a by-product of thesulphate process for the making of wood pulp. It is sold commercially in the crude or in refined forms and consists essentially of rosin acids and higher fatty acids; the content of fatty acids being slightly higher in the refined tall-oils. Typical talloils produced in the United States may contain in respectto crude talloil, from 30% to 65% of rosin acids and from 40% to 60% of fatty acids, with up to of unsaponifiable material, and refined and bleached (or v distilled) talloils may contain, for example, from to of rosin acids and from 50% to 60% I of fatty acids, with up to 10% of unsaponifiable mass a quantity of aqueous potassium hydroxide sufiicient to completely neutralize the acids of the talloil and the saponification carried out as before. The aliphatic alcohol is not separated from the talloil soap. .It is used in amounts suflicient to form an easily stirrable reaction mass in the saponification.

The following specific example is illustrative of the preparation of the mixed talloil soap compositions useful as stabilizing agents in accordance with the invention. Parts are by weight.

Example 1 1600 parts of a refined talloil, 600 parts of isobutanol and 32 parts of diethylenetriamine are placed in a reaction vessel equipped with a stirrer, reflux condenser and thermometer. Th mixture is stirred at room temperature until the partial saponification of the talloil is complete. While stirring at room temperature or at slightly elevated temperatures due to the heat of reaction from the previous saponification, there is added to the soap mass, 500 pa s of an aqueous 50% potassium hydroxide solution and the stirring continued at these temperatures until saponification of the talloil is complete. The product is a dark thick liquid soluble in both water and gasoline hydrocarbons.

I have further found that when, in addition to the aforementioned soap compositions, there is also blended with the iron carbonyl a minor proportion thereon of an aliphatic monocarboxylic acid, a still greater improvement in th stability of the iron carbonyl to light can be obtained. The increase in stability of the iron pentacarbonyl due to the addition of the aliphatic acid may arise from the acidification of the talloil soap thereby, the soap otherwise being a neutral or alkaline composition.

Concentrates of stabilized iron carbonyl may be prepared by dissolving the talloil soap comganic solvent.

The following is a specific example or a stabilibzed iron carbonyl which can be prepared in accordance with the invention. Parts are by volume:

Parts Iron carbonyl 30 Gasoline 36 Talloil soap composition t 7.5 Oleic acid 3.0

In place of the oleic acid a like amount of naphthenic acids, crotonic acid, palmitic acid, stearic acid or riclnoleic acid may be used.

As various other embodiments of the invention will occur to those skilled in the art, it is not intended that the scope of the patent be limited except as is required by the prior art and the appended claims.

I claim:

1. Iron carbonyl blended, through an organic solvent, with at least 5%. of its volume of a talloil soap composition, obtained by partially saponifying talloil in a liquid diluent aliphatic alcohol of at least 3 carbon atoms, with an alkylene polyamine selected from the group consisting of the polyalkylene polyamines and the hydrcxyalkyl alkylene polyamines, and completing the seaponiiication with potassium hydroxide.

2.- Iron carbonyl blended, through a hydrocarbon solvent, with at least 5% of its volume of a talloil soap composition, obtained by partially saponifying talloil in a liquid diluent aliphatic alcohol of at least 3 carbon atoms, with an alkylene polyamine selected from the group consisting of the polyaikylene polyamines and the hydroxyalkyl alkylene polyamines, and completing the saponification with potassium hydroxide.

3. A composition as defined in claim 2 wherein the polyalkylene polyamine from which the mixed talloil soap is partly prepared is diethylenetrlamine.

4. A composition as defined in claim 3, wherein the alcohol is isobutanol.

5. A composition as definedin claim 2, in which is additionally blended a minor proportion on the iron carbonyl of an aliphatic monocarboxylic acid.

6. A composition as defined in claim 1, in which is additionally blended a minor proportion on the iron carbonyl of a long chain fatty acid.

7. A composition as defined in claim 2, in which is additionally blended a minor proportion on the iron carbonyl 01 along chain fatty acid.

ROBERT E. CHRIST.

REFERENCES CITED The following references are of record in the file of this patent? UNITED STATES PATENTS Number Name Date 1,940,096 Mueller-Cunradi"..- Dec. 19, 1933 2,140,627 Hocking Dec. 20, 1938 

1. IRON CARBONYL BLENDED, THROUGH AN ORGANIC SOLVENT, WITH AT LEAST 5% OF ITS VOLUME OF A TALLOIL SOAP COMPOSITION, OBTAINED BY PARTIALLY SAPONIFYING TALLOIL IN A LIQUID DILUENT ALIPHATIC ALCOHOL OF AT LEAST 3 CARBON ATOMS, WITH AN ALKYLENE POLYAMINE SELECTED FROM THE GROUP CONSISTING OF THE POLYALKYLENE POLYAMINES AND THE HYDROXYALKYL ALKYLENE POLYAMINES, AND COMPLETING THE SEAPONIFICATION WITH POTASSIUM HYDROXIDE. 